EP0490232B1 - Device for detecting marked mineral oils - Google Patents
Device for detecting marked mineral oils Download PDFInfo
- Publication number
- EP0490232B1 EP0490232B1 EP91120739A EP91120739A EP0490232B1 EP 0490232 B1 EP0490232 B1 EP 0490232B1 EP 91120739 A EP91120739 A EP 91120739A EP 91120739 A EP91120739 A EP 91120739A EP 0490232 B1 EP0490232 B1 EP 0490232B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- substance
- container
- mineral oils
- metering
- detection
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 239000002480 mineral oil Substances 0.000 title claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 23
- 239000003480 eluent Substances 0.000 claims abstract description 6
- 238000005070 sampling Methods 0.000 claims abstract description 5
- 239000003921 oil Substances 0.000 claims description 10
- 238000001514 detection method Methods 0.000 abstract description 19
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 9
- 235000010446 mineral oil Nutrition 0.000 abstract description 9
- 239000012071 phase Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 239000000975 dye Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/26—Oils; Viscous liquids; Paints; Inks
- G01N33/28—Oils, i.e. hydrocarbon liquids
- G01N33/2835—Specific substances contained in the oils or fuels
- G01N33/2882—Markers
Definitions
- the invention relates to a device for the detection of marked mineral oils.
- Mineral oils which are subject to a lower purchase tax compared to fuels, for example heating oil, are marked for visual recognition during checks by the tax authorities against misuse with another substance, for example furfurol, which gives a characteristic color when reacted with a detection reagent.
- another substance for example furfurol
- furfurol which gives a characteristic color when reacted with a detection reagent.
- the marking substance is not present in the prescribed amount, but in a lower concentration, for example if the marked mineral oil has been manipulated for the purpose of changing its original quality or for its intended tax purposes. Such manipulation occurs, for example, when fuel oil favored for tax purposes is mixed with diesel fuel and thus diesel vehicles are operated.
- the marking substance originally in the heating oil is then only present in the mixture in a low concentration.
- Interfering substances can be natural or synthetic substances that are added to the mineral oil product or are present due to its origin and impair the detection reaction.
- a second phase which is immiscible with the heating oil, is often formed in a detection reaction. In this phase, the marker is extracted and, with the detection reagent, gives the color reaction that is characteristic. If this characteristic color reaction is not observed when carrying out the detection, it can be concluded that the mineral oil is not marked.
- the disturbance of the detection reaction can also be caused by substances present in the mineral oil, which are extracted from the detection reagent in the second phase. Most of these products have their own color or even react with the detection reagent in a color reaction, which makes it difficult to identify the marking material properly.
- the present invention is therefore based on the object of developing a device for the detection of labeled mineral oils, with the aid of which mineral oil-marking substances can be reliably detected even at a reduced concentration in the oil or in its mixture and in the presence of interfering substances, the possible uses compared to the known ones Facilities should be improved.
- the device achieving the object is characterized according to the invention by a device for sampling and metering an oil sample to be examined, a container for a substance that adsorbs the marking substance, which can be connected to a metering device for an eluent, and one arranged below the container outlet exchangeable collecting container for the oil sample or the eluate.
- a sample of the mineral oil to be examined is taken from a tank or canister with the aid of a metering pump 1 via a hose line 6, which sample is then passed through a container 2 in which there is a substance adsorbing the marking substance of the mineral oil.
- Various products can be used for this, for example products customary in analytics for column chromatography. These can be of an inorganic nature, such as different qualities of silica gel or diatomaceous earth or alumina or magnesium silicate. However, products of an organic nature are also suitable, such as those used in normal or reverse phase extraction.
- the marking substance is passed through Rinsing the adsorbent substance with a suitable eluent selectively detached from this substance and thereby reaches the collecting container 3 in the eluate.
- the connection between the metering pump 1 and the container 2 consists of a T-shaped connecting part 4, for example a three-way valve, on its side Input via a metering device 5, for example a piston pump, a reservoir with the eluent is connected.
- the amount of detection reagent necessary for the detection reaction may already be present in the collecting container 3. However, it is equally possible to add the detection reagent to the eluate in the collecting container. After the contents of the collecting container have been mixed, the color reaction begins if the marking substance is present.
- the eluate and detection reagent can form one or two phases with one another.
- a further embodiment of the device according to the invention consists in that a suction cylinder 8 is used instead of the metering pump, with which a sample can be drawn from a tank via the hose line 6. After sampling, the suction cylinder is placed on the inlet opening of the connecting part 4 and the oil sample is pushed through the container by advancing the piston 9 in the cylinder.
- the device described above extends the possible uses of the detection method described at the outset, in particular mobile use and implementation with trained personnel are possible.
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Pathology (AREA)
- General Chemical & Material Sciences (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Fats And Perfumes (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Sampling And Sample Adjustment (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Lubricants (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
- Geophysics And Detection Of Objects (AREA)
Abstract
Description
Die Erfindung betrifft eine Vorrichtung zum Nachweis markierter Mineralöle.The invention relates to a device for the detection of marked mineral oils.
Mineralöle, die gegenüber Kraftstoffen mit einer niedrigeren Kaufsteuer belastet sind, beispielsweise Heizöl, werden zur optischen Erkennbarkeit bei Kontrollen der Steuerbehörde gegen Mißbrauch mit einem weiteren Stoff, beispielsweise Furfurol markiert, der bei Reaktion mit einem Nachweisreagenz eine charakteristische Farbe ergibt. In der praktischen Anwendung kann es vorkommen, daß im Mineralöl vorhandene Stoffe die Nachweisreaktion stören. Eine Störung wird dann als solche empfunden, wenn die erwartete charakteristische Farbreaktion nicht eindeutig feststellbar ist. Dies ist insbesondere der Fall, wenn der Markierstoff nicht in der vorgeschriebenen Menge, sondern in geringerer Konzentration vorliegt, zum Beispiel wenn das markierte Mineralöl zum Zweck der Veränderung seiner ursprünglichen Qualität oder seiner steuerlich vorgesehenen Bestimmung manipuliert wurde. Eine solche Manipulation liegt zum Beispiel vor, wenn stuerlich begünstigtes Heizöl mit Dieselkraftstoff vermischt wird und damit Dieselfahrzeuge betrieben werden. Der ursprünglich im Heizöl befindliche Markierstoff ist dann nur noch in geringer Konzentration im Gemisch vorhanden.Mineral oils, which are subject to a lower purchase tax compared to fuels, for example heating oil, are marked for visual recognition during checks by the tax authorities against misuse with another substance, for example furfurol, which gives a characteristic color when reacted with a detection reagent. In practical application, it can happen that substances present in the mineral oil interfere with the detection reaction. A disturbance is perceived as such if the expected characteristic color reaction cannot be clearly determined. This is particularly the case if the marking substance is not present in the prescribed amount, but in a lower concentration, for example if the marked mineral oil has been manipulated for the purpose of changing its original quality or for its intended tax purposes. Such manipulation occurs, for example, when fuel oil favored for tax purposes is mixed with diesel fuel and thus diesel vehicles are operated. The marking substance originally in the heating oil is then only present in the mixture in a low concentration.
Störende Stoffe können natürliche oder synthetische Stoffe sein, die dem Mineralölprodukt zugesetzt oder aufgrund seiner Herkunft vorhanden sind und die Nachweisreaktion beeinträchtigen. Häufig wird bei einer Nachweisreaktion eine zweite, mit dem Heizöl nicht mischbare Phase gebildet. In dieser Phase wird der Markierstoff extrahiert und ergibt mit dem Nachweisreagenz die Farbreaktion, die charakteristisch ist. Wird bei der Durchführung des Nachweises diese charakteristische Farbreaktion nicht beobachtet, kann der Schluß gezogen werden, daß das Mineralöl nicht markiert ist.Interfering substances can be natural or synthetic substances that are added to the mineral oil product or are present due to its origin and impair the detection reaction. A second phase, which is immiscible with the heating oil, is often formed in a detection reaction. In this phase, the marker is extracted and, with the detection reagent, gives the color reaction that is characteristic. If this characteristic color reaction is not observed when carrying out the detection, it can be concluded that the mineral oil is not marked.
Die Störung der Nachweisreaktion kann ferner durch im Mineralöl vorhandene Stoffe hervorgerufen werden, welche von dem Nachweisreagenz in die zweite Phase mitextrahiert werden. Meistens besitzen diese Produkte eine Eigenfarbe oder reagieren selbst in einer Farbreaktion mit dem Nachweisreagenz, wodurch das einwandfreie Identifizieren des Markierstoffes erschwert wird.The disturbance of the detection reaction can also be caused by substances present in the mineral oil, which are extracted from the detection reagent in the second phase. Most of these products have their own color or even react with the detection reagent in a color reaction, which makes it difficult to identify the marking material properly.
Aus der Patentschrift US-A-4 918 020 ist ein Verfahren zur Bestimmung von Kohlenwasserstoffbrennstoffe markierenden Farbstoffen bekannt, wobei der Farbstoff vom Brennstoff mittels einer den Farbstoff adsorbierenden Festphase extrahiert, von der Festphase mit einer Eluierflüssigkeit gelöst und mit einem Nachweisreagenz zur Farbindikation gemischt wird. Für die Durchführung dieses Verfahrens ist ein Analyseablauf in 15 Stufen unter Zuhilfenahme zahlreicher in Analyselabors üblicher Laborgeräte beschrieben. Der damit verbundene hohe Arbeits- und Zeitaufwand sowie die Erfordernis eines umfangreichen Laborplatzes schränkt die Einsatzmöglichkeiten des Verfahrens jedoch ein.From the patent US-A-4 918 020 a method for the determination of hydrocarbon fuel-marking dyes is known, wherein the dye is extracted from the fuel by means of a solid phase adsorbing the dye, dissolved from the solid phase with an eluting liquid and mixed with a detection reagent for color indication. For the implementation of this method, an analysis process in 15 stages is described with the aid of numerous laboratory devices that are customary in analysis laboratories. The associated high work and time expenditure as well as the requirement of an extensive laboratory space, however, limit the possible uses of the method.
Vorliegender Erfindung liegt daher die Aufgabe zugrunde, eine Vorrichtung zum Nachweis markierter Mineralöle zu entwickeln, mit deren Hilfe Mineralöl markierende Stoffe auch bei verminderter Konzentration im Öl bzw. in dessen Gemisch und bei Vorhandensein störender Stoffe sicher nachgewiesen werden können, wobei die Einsatzmöglichkeiten gegenüber den bekannten Einrichtungen verbessert sein sollen.The present invention is therefore based on the object of developing a device for the detection of labeled mineral oils, with the aid of which mineral oil-marking substances can be reliably detected even at a reduced concentration in the oil or in its mixture and in the presence of interfering substances, the possible uses compared to the known ones Facilities should be improved.
Die die Aufgabe lösende Vorrichtung ist gemäß der Erfindung gekennzeichnet durch eine Einrichtung zur Probenahme und Dosierung einer zu untersuchenden Ölprobe, einen daran anschließbaren Behälter für einen den Markierstoff adsorbierenden Stoff, der mit einer Dosiereinrichtung für eine Eluiermittel verbindbar ist, und durch einen unterhalb des Behälterausgangs angeordneten austauschbaren Auffangbehälter für die Ölprobe bzw. das Eluat.The device achieving the object is characterized according to the invention by a device for sampling and metering an oil sample to be examined, a container for a substance that adsorbs the marking substance, which can be connected to a metering device for an eluent, and one arranged below the container outlet exchangeable collecting container for the oil sample or the eluate.
Die Erfindung ist anhand eines in der Zeichnung schematisch dargestellten Ausführungsbeispiel nachfolgend näher beschrieben.The invention is described below with reference to an embodiment shown schematically in the drawing.
Von dem zu untersuchenden Mineralöl wird aus einem Tank oder Kanister mit Hilfe einer Dosierpumpe 1 über eine Schlauchleitung 6 eine Probe genommen, die anschließend durch einen Behälter 2 geleitet wird, in dem sich ein den Markierstoff des Mineralöls adsorbierender Stoff befindet. Hierfür können verschiedene Produkte eingesetzt werden, beispielsweise in der Analytik für die Säulenchromatographie übliche Produkte. Diese können anorganischer Natur sein, wie zum Beispiel verschiedene Qualitäten von Silicagel oder Kieselgur oder Alumina oder Magnesiumsilikat. Aber auch Produkte organischer Natur kommen in Betracht, wie sie zum Beispiel in der Normal- oder Umkehrphasen-Extraktion verwendet werden.A sample of the mineral oil to be examined is taken from a tank or canister with the aid of a
Nach dem Entfernen des durch den Behälter 2 gelaufenen Mineralöls aus einem unter diesem angeordneten Auffangbehälter 3 oder nach Aufstellen eines neuen Behälters 3 wird der Markierstoff durch Spülen des adsorbierenden Stoffes mit einem geeigneten Eluiermittel selektiv von diesem Stoff gelöst und gelangt dabei im Eluat in den Auffangbehälter 3. Hierzu besteht die Verbindung zwischen der Dosierpumpe 1 und dem Behälter 2 aus einem T-förmigen Verbindungsteil 4, beispielsweise einem Dreiwegehahn, an dessen seitlichem Eingang über eine Dosiereinrichtung 5, beispielsweise eine Kolbenpumpe, ein Vorratsbehälter mit dem Eluiermittel angeschlossen ist.After the mineral oil that has passed through the
Im Auffangbehälter 3 kann bereits die für die Nachweisreaktion notwendige Menge an Nachweisreagenz vorhanden sein. Es ist aber ebenso gut möglich, das Nachweisreagenz nachträglich dosiert dem Eluat im Auffangbehälter zuzugeben. Nach Durchmischen des Auffangbehälterinhalts setzt bei Vorhandensein des Markierstoffes die Farbreaktion ein. Eluat und Nachweisreagenz können dabei eine oder zwei Phasen miteinander bilden.The amount of detection reagent necessary for the detection reaction may already be present in the collecting
Eine weitere Ausführungsform der erfindungsgemäßen Vorrichtung dann darin bestehen, daß anstelle der Dosierpumpe ein Saugzylinder 8 verwendet wird, mit dem über die Schlauchleitung 6 eine Probe aus einem Tank gezogen werden kann. Nach der Probenahme wird der Saugzylinder auf die Eingangsöffnung des Verbindungsteils 4 gesetzt und die Ölprobe durch Vorschieben des Kolbens 9 im Zylinder durch den Behälter gedrückt.A further embodiment of the device according to the invention then consists in that a
Die vorstehend beschriebene Vorrichtung erweitert die Einsatzmöglichkeiten des eingangs beschriebenen Nachweisverfahrens, wobei insbesondere ein mobiler Einsatz sowie die Durchführung mit angelerntem Personal möglich sind.The device described above extends the possible uses of the detection method described at the outset, in particular mobile use and implementation with trained personnel are possible.
Claims (2)
- Apparatus for detecting marked mineral oils, which comprises a means (1) for sampling and metering an oil sample to be investigated, a container (2) for a substance which adsorbs the marking substance, which can be connected to said means and to a metering means (5) for an eluent, and an interchangeable collecting tank (3) for the oil sample or eluate, which tank is arranged underneath the container outlet.
- Apparatus as claimed in claim 1, wherein the entrance of the container (2) is connected by means of a three-way valve (4) to the means (1) for sampling and metering the oil sample and to the metering means (5) for the eluent.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE4040080 | 1990-12-14 | ||
DE4040080A DE4040080A1 (en) | 1990-12-14 | 1990-12-14 | METHOD AND DEVICE FOR DETECTING MARKED MINERAL OILS |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0490232A1 EP0490232A1 (en) | 1992-06-17 |
EP0490232B1 true EP0490232B1 (en) | 1995-08-23 |
Family
ID=6420397
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP91120739A Expired - Lifetime EP0490232B1 (en) | 1990-12-14 | 1991-12-03 | Device for detecting marked mineral oils |
Country Status (10)
Country | Link |
---|---|
EP (1) | EP0490232B1 (en) |
AT (1) | ATE126890T1 (en) |
DE (2) | DE4040080A1 (en) |
DK (1) | DK0490232T3 (en) |
ES (1) | ES2075313T3 (en) |
FI (1) | FI102786B (en) |
IE (1) | IE68316B1 (en) |
NO (1) | NO301303B1 (en) |
PT (1) | PT99811B (en) |
YU (1) | YU192191A (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114280254B (en) * | 2021-12-29 | 2024-04-30 | 河北香宇肉类制品有限公司 | Edible oil detection device and method |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4209302A (en) * | 1979-05-10 | 1980-06-24 | Morton-Norwich Products, Inc. | Marker for petroleum fuels |
US4514503A (en) * | 1982-09-01 | 1985-04-30 | Morton Norwich Products | Reagent and process for detecting furfural in petroleum products |
FI84346C (en) * | 1983-12-16 | 1991-11-25 | Thiokol Morton Inc | Colored labeling compounds for petroleum products |
DE3731458A1 (en) * | 1987-09-18 | 1989-03-30 | Basf Ag | MARKING MIXTURE FOR LABELING MINERAL OIL PRODUCTS AND MARKED MINERAL OIL PRODUCTS |
GB8802237D0 (en) * | 1988-02-02 | 1988-03-02 | Shell Int Research | Detection of chemicals by immunoassay |
US4918020A (en) * | 1989-03-21 | 1990-04-17 | Atlantic Richfield Company | Analyzing marker dyes in liquid hydrocarbon fuels |
-
1990
- 1990-12-14 DE DE4040080A patent/DE4040080A1/en not_active Withdrawn
-
1991
- 1991-11-28 FI FI915614A patent/FI102786B/en active
- 1991-12-03 AT AT91120739T patent/ATE126890T1/en not_active IP Right Cessation
- 1991-12-03 ES ES91120739T patent/ES2075313T3/en not_active Expired - Lifetime
- 1991-12-03 DE DE59106312T patent/DE59106312D1/en not_active Expired - Lifetime
- 1991-12-03 EP EP91120739A patent/EP0490232B1/en not_active Expired - Lifetime
- 1991-12-03 DK DK91120739.7T patent/DK0490232T3/en active
- 1991-12-11 YU YU192191A patent/YU192191A/en unknown
- 1991-12-13 IE IE435191A patent/IE68316B1/en not_active IP Right Cessation
- 1991-12-13 NO NO914941A patent/NO301303B1/en not_active IP Right Cessation
- 1991-12-13 PT PT99811A patent/PT99811B/en not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
NO914941D0 (en) | 1991-12-13 |
NO914941L (en) | 1992-06-15 |
DK0490232T3 (en) | 1995-09-25 |
ES2075313T3 (en) | 1995-10-01 |
DE59106312D1 (en) | 1995-09-28 |
IE914351A1 (en) | 1992-06-17 |
NO301303B1 (en) | 1997-10-06 |
FI915614A (en) | 1992-06-15 |
DE4040080A1 (en) | 1992-06-17 |
ATE126890T1 (en) | 1995-09-15 |
PT99811A (en) | 1994-01-31 |
YU192191A (en) | 1994-01-20 |
FI102786B1 (en) | 1999-02-15 |
FI102786B (en) | 1999-02-15 |
FI915614A0 (en) | 1991-11-28 |
IE68316B1 (en) | 1996-06-12 |
EP0490232A1 (en) | 1992-06-17 |
PT99811B (en) | 1999-06-30 |
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